Determination of pharmaceuticals in drinking water by CD-modified MEKC: separation optimization using experimental design.
A suite of 12 widely used pharmaceuticals (ibuprofen, diclofenac, naproxen, bezafibrate, gemfibrozil, ofloxacin, norfloxacin, carbamazepine, primidone, sulphamethazine, sulphadimethoxine and sulphamethoxazole) commonly found in environmental waters were separated by highly sulphated CD-modified MEKC (CD-MEKC) with UV detection. An experimental design method, face-centred composite design, was employed to minimize run time without sacrificing resolution. Using an optimized BGE composed of 10 mM ammonium hydrogen phosphate, pH 11.5, 69 mM SDS, 6 mg/mL sulphated beta-CD and 8.5% v/v isopropanol, a separation voltage of 30 kV and a 48.5 cm x 50 microm id bare silica capillary at 30 degrees C allowed baseline separation of the 12 analytes in a total analysis time of 6.7 min. Instrument LODs in the low milligram per litre range were obtained, and when combined with offline preconcentration by SPE, LODs were between 4 and 30 microg/L.
Drover
Vincent J
VJ
Department of Chemistry, Memorial University of Newfoundland, St. John's, NL, Canada.
Bottaro
Christina S
CS
D000818:Animals; D002138:Calibration; D020374:Chromatography, Micellar Electrokinetic Capillary / Q000295:instrumentation / Q000379:methods*; D006801:Humans; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results; D012107:Research Design; D013056:Spectrophotometry, Ultraviolet / Q000295:instrumentation / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification; D014881:Water Supply
D004364:Pharmaceutical Preparations; D014874:Water Pollutants, Chemical